Preparation method of pollution-free low-cost lithium manganese ferric phosphate crystal material

A technology of lithium iron manganese phosphate and crystalline materials, applied in phosphorus compounds, inorganic chemistry, non-metallic elements, etc., can solve the problems of unsolved safety problems, limited energy density, and difficulty in charging and discharging. The effect of low synthesis cost, increased synthesis cost, and improved overall level

Active Publication Date: 2018-08-17
南阳逢源新能源科技有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although the energy density of ternary materials is high, the safety problem has not been well solved so far, and its preparation requires a large amount of rare element cobalt
Although the traditional lithium iron phosphate has a series of advantages such as environmental friendliness, safety, low cost, and long life, its 3.2V voltage limits its energy density.
Although lithium manganese phosphate has an olivine stable structure similar to lithium iron phosphate and has a voltage platform of 4.1V, its conductivity is particularly poor and it is an insulator, which makes it difficult to effectively charge and discharge, which limits its commercial use.

Method used

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  • Preparation method of pollution-free low-cost lithium manganese ferric phosphate crystal material
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  • Preparation method of pollution-free low-cost lithium manganese ferric phosphate crystal material

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Effect test

Embodiment 1

[0032] A preparation process of pollution-free and low-cost lithium manganese iron phosphate crystal material, comprising the following steps:

[0033] 1) Weigh iron powder, manganese powder and phosphoric acid according to the molar ratio of 0.3:0.7:1, and the diluted concentration of phosphoric acid is 40%;

[0034] 2) Put the substance weighed in step 1) into the acid-resistant reactor to control the temperature of the reaction system between 30°C, feed oxygen to start the pre-reaction, and the reaction time is 24 hours;

[0035] 3) Step 2) Add lithium hydroxide solution after the reaction, lithium hydroxide and phosphoric acid are mixed at a ratio of 1:1, after mixing evenly, the precursor is transferred into an autoclave, and the reaction is sealed. The temperature during the synthesis process is 120-260 ° C, high pressure The pressure of the kettle is 0.2-4.7MPa, the whole reaction process is continuously dispersed and stirred, the reaction time is controlled within 3-24...

Embodiment 2

[0039] A preparation process of pollution-free and low-cost lithium manganese iron phosphate crystal material, comprising the following steps:

[0040] 1) Weigh iron powder, manganese powder, and phosphoric acid according to the molar ratio of 0.5:0.5:1-1.2, and the diluted concentration of phosphoric acid is 35%;

[0041] 2) Put the substance weighed in step 1) into the acid-resistant reactor to control the temperature of the reaction system between 25 and 80°C, feed oxygen to start the pre-reaction, and the reaction time is 18 hours;

[0042] 3) Step 2) After the reaction, add lithium hydroxide solution, lithium hydroxide and phosphoric acid are mixed at a ratio of 1-1.2:1, after mixing evenly, the precursor is transferred into an autoclave, and the reaction is sealed. The temperature during the synthesis process is 120-260°C , the pressure of the autoclave is 0.2-4.7MPa, the whole reaction process is continuously dispersed and stirred, the reaction time is controlled within...

Embodiment 3

[0046] A preparation process of pollution-free and low-cost lithium manganese iron phosphate crystal material, comprising the following steps:

[0047] 1) Weigh iron powder, manganese powder, and phosphoric acid according to the molar ratio of 0.4:0.6:1-1.2, and the diluted concentration of phosphoric acid is 30%;

[0048] 2) Put the substance weighed in step 1) into the acid-resistant reactor to control the temperature of the reaction system between 25 and 80°C, feed oxygen to start the pre-reaction, and the reaction time is 18 hours;

[0049]3) Step 2) After the reaction, add lithium hydroxide solution, lithium hydroxide and phosphoric acid are mixed at a ratio of 1-1.2:1, after mixing evenly, the precursor is transferred into an autoclave, and the reaction is sealed. The temperature during the synthesis process is 120-260°C , the pressure of the autoclave is 0.2-4.7MPa, the whole reaction process is continuously dispersed and stirred, the reaction time is controlled within ...

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Abstract

The invention discloses a preparation method of a pollution-free low-cost lithium manganese ferric phosphate crystal material. The preparation method includes following steps: selecting iron powder and manganese powder high in purity, wherein granularity is selected from 20-20000 meshes; taking the manganese powder, the iron powder, phosphoric acid and a lithium source solution according to a certain mass ratio, diluting, putting them into an acid-resistant reactor, and stirring to enable the iron powder, the manganese powder and the phosphoric acid to be in sufficient reaction; adding the lithium source solution into obtained reaction precursor size, and sufficiently stirring, wherein the lithium source solution is soluble lithium source lithium hydroxide or lithium acetate; transferringobtained size into a reaction kettle, and starting hydrothermal reaction; performing solid-liquid separation on size obtained after reaction, and subjecting solid lithium manganese ferric phosphate which is separated out to clathration carbonization annealing treatment to obtain the lithium manganese ferric phosphate crystal material. Compared with the prior art, the preparation method has the advantages that cost is low, process operation is convenient, the material is high in commercial value, the preparation process is free of pollution, and current requirements on environment protection are met.

Description

technical field [0001] The invention relates to the technical field of chemical material synthesis, in particular to a preparation process of a pollution-free and low-cost lithium manganese iron phosphate crystal material. Background technique [0002] With the rapid development of electric vehicles and the gradual expansion of 3C and energy storage market demand, higher requirements are placed on the energy density of materials. Although the energy density of ternary materials is high, the safety problem has not been well resolved so far, and its preparation requires a large amount of rare element cobalt. Although traditional lithium iron phosphate has a series of advantages such as environmental friendliness, safety, low cost, and long life, its 3.2V voltage limits its energy density. Although lithium manganese phosphate has an olivine stable structure similar to lithium iron phosphate and has a voltage platform of 4.1V, its electrical conductivity is particularly poor, a...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B25/45H01M4/58
CPCH01M4/5825C01B25/45C01P2006/40C01P2004/62C01P2004/01C01P2002/72Y02E60/10
Inventor 孙青林魏宏政贾庆煜白兵
Owner 南阳逢源新能源科技有限公司
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